CN107828410B - A kind of preparation method of carbon quantum dot-molecular imprinting composite material and the remaining method of pesticide mesotrione is analyzed using its - Google Patents
A kind of preparation method of carbon quantum dot-molecular imprinting composite material and the remaining method of pesticide mesotrione is analyzed using its Download PDFInfo
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- CN107828410B CN107828410B CN201711055068.XA CN201711055068A CN107828410B CN 107828410 B CN107828410 B CN 107828410B CN 201711055068 A CN201711055068 A CN 201711055068A CN 107828410 B CN107828410 B CN 107828410B
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- quantum dot
- carbon quantum
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- mesotrione
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 87
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 86
- 239000005578 Mesotrione Substances 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 63
- KPUREKXXPHOJQT-UHFFFAOYSA-N mesotrione Chemical compound [O-][N+](=O)C1=CC(S(=O)(=O)C)=CC=C1C(=O)C1C(=O)CCCC1=O KPUREKXXPHOJQT-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000575 pesticide Substances 0.000 title claims abstract description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 239000006185 dispersion Substances 0.000 claims abstract description 22
- 239000002096 quantum dot Substances 0.000 claims abstract description 22
- 238000010791 quenching Methods 0.000 claims abstract description 19
- 230000000171 quenching effect Effects 0.000 claims abstract description 19
- 238000004458 analytical method Methods 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 84
- 239000012498 ultrapure water Substances 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 238000012360 testing method Methods 0.000 claims description 16
- 230000005284 excitation Effects 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 12
- 239000012265 solid product Substances 0.000 claims description 11
- 239000007795 chemical reaction product Substances 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 240000002044 Rhizophora apiculata Species 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 239000005864 Sulphur Substances 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- RMFGNMMNUZWCRZ-UHFFFAOYSA-N Humulone Natural products CC(C)CC(=O)C1=C(O)C(O)(CC=C(C)C)C(O)=C(CC=C(C)C)C1=O RMFGNMMNUZWCRZ-UHFFFAOYSA-N 0.000 claims description 2
- VMSLCPKYRPDHLN-NRFANRHFSA-N humulone Chemical compound CC(C)CC(=O)C1=C(O)C(CC=C(C)C)=C(O)[C@@](O)(CC=C(C)C)C1=O VMSLCPKYRPDHLN-NRFANRHFSA-N 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 235000004936 Bromus mango Nutrition 0.000 claims 1
- 240000007228 Mangifera indica Species 0.000 claims 1
- 235000014826 Mangifera indica Nutrition 0.000 claims 1
- 235000009184 Spondias indica Nutrition 0.000 claims 1
- 238000010828 elution Methods 0.000 claims 1
- 125000004494 ethyl ester group Chemical group 0.000 claims 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000008077 Ruellia tuberosa Species 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000344 molecularly imprinted polymer Polymers 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000009870 specific binding Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Optics & Photonics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Molecular Biology (AREA)
- Inorganic Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Carbon And Carbon Compounds (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
A kind of preparation method of carbon quantum dot-molecular imprinting composite material and the remaining method of pesticide mesotrione is analyzed using its, it is related to a kind of preparation method of carbon quantum dot-molecular imprinting composite material and the analysis method to pesticide mesotrione.Present invention aim to address existing method is long to mesotrione analysis time, the low and quantum dot molecular imprinting composite material synthetic method of selectivity is at high cost, the problem of causing serious pollution to the environment.Preparation method: one, carbon quantum dot is prepared；Two, modified carbon quantum dot；Three, molecular engram obtains carbon quantum dot-molecular imprinting composite material.Analysis method: one, dispersion liquid is prepared；Two, control group fluorescence intensity is detected；Three, quenching constant K is determinedsv；Four, sample to be tested is detected, the concentration Q of mesotrione in sample to be tested is calculatedu.Present invention is mainly used for pesticide mesotrione residuals in analysis environmental water sample.
Description
Technical field
The present invention relates to a kind of preparation method of carbon quantum dot-molecular imprinting composite material and to pesticide mesotrione
Analysis method.
Background technique
Carbon quantum dot is referred to using C as main component, and combines a kind of similar semiconductor amount of the elements such as H, O, N composition
The material with fluorescent characteristic of son point, particle size is from a few nanometers to tens of nanometers etc..With hypotoxicity, good life
Object compatibility and photostability.The primary raw material for preparing carbon quantum dot at this stage is graphene, carbon nanotube etc..Such raw material
It is mostly more expensive, and product needs just to can guarantee that carbon quantum dot is stablized by means such as strong acid reflow treatment or surface modifications
Optical property, limit the large-scale production and practical application of carbon quantum dot.Therefore, biomass precursor preparation carbon amounts is developed
Son point has a good application prospect.Such as it is " a kind of using cotton as the side of raw material hydrothermal synthesis carbon quantum dot in disclosed patent
Method " (application number: 201410424098.3) and patent " a kind of preparation method of luminescence generated by light carbon quantum dot " (application number:
201310487328.6) all once used cotton and milk for the method for raw material hydrothermal synthesis carbon quantum dot.
Molecular imprinting technology refers to polymer of the creation to a certain specific template molecule with specific binding site
Process.Molecular imprinting technology is a kind of novel preparation technology of multi-crossed disciplines, analogue antigen-antibody recognition mechanism, synthesis
With fixing hole size and shape and having the polymer of the functional group centainly to put in order, it can be to template molecule body
Reveal special selectivity and good recognition capability.If can be incorporated into fluorescent material in molecularly imprinted polymer can make its tool
There are fluorescent emission properties again while having highly selective.Such as " one kind is based on core-shell quanta dots molecular engram to disclosed patent
Polymer and application thereof " (application number: 201410520007.6).Although it is multiple that quantum dot-molecular engram is successfully prepared in the invention
Condensation material, but organic solvent and cadmium metal compound are largely used in preparation process, synthesis cost is high and causes serious pollution to the environment, and limits
The practical application of quantum dot molecular imprinting composite material.
Mesotrione is the controlling selection herbicide before the emergence for broad-leaved in corn and meadow weeds and after emergence.
Due to its excellent Weeds distribution property, many growers control the weeds in rice field using mesotrione.Although nitre sulphur grass
Ketone plays an important role in the practice of agriculture, but has toxicity to nontarget organism body.It has negative effect to the growth of microalgae,
And the structure and function of aquatic ecosystem may be influenced.The common analysis method to mesotrione, such as high performance liquid chromatography
It needs to expend a large amount of organic solvent and analysis time is longer (being greater than 1h comprising pretreatment time), be not suitable for a large amount of samples of processing
Product, higher cost.
Summary of the invention
Present invention aim to address existing method is long to mesotrione analysis time, the low and quantum dot-point of selectivity
Sub- trace method for synthesizing composite material is at high cost, and the problem of causing serious pollution to the environment, and it is multiple to provide a kind of carbon quantum dot-molecular engram
The preparation method of condensation material and the remaining method of pesticide mesotrione is analyzed using its.
A kind of preparation method of carbon quantum dot-molecular imprinting composite material, is specifically realized by the following steps:
One, it prepares carbon quantum dot: mangrove bark being put into polytetrafluoroethyllining lining first, high purity water is added and is uniformly mixed,
It is put into stainless steel cauldron after capping, reaction kettle is sealed, be then placed in air dry oven, be 180 DEG C~220 in temperature
3h~7h is reacted at DEG C, after being cooled to room temperature, obtains reaction product, and the micropore filtering film for being 20 μm~40 μm using aperture is to anti-
It answers product to be filtered, obtains lurid filtrate, which is carbon quantum dot solution；It is described in step 1
The quality of mangrove bark and the volume ratio of high purity water are 1g:(10~20) mL；
Two, modified carbon quantum dot: 3- aminopropyl triethoxysilane is added into carbon quantum dot solution, low whipping speed is
100rpm~300rpm and temperature are that 20h~30h is reacted at 50 DEG C~70 DEG C, and solution after being reacted exists solution after reaction
Revolving speed be 5000rpm~7000rpm under the conditions of be centrifuged 5min~10min, isolated supernatant, using ether to supernatant into
Row extraction 2~4 times, obtains carbon modified quantum dot solution；3- aminopropyl triethoxysilane and carbon quantum described in step 2
The volume ratio of point solution is 1:(22~28)；
Three, molecular engram: mesotrione is put into container, and dehydrated alcohol is then added, and is 35 DEG C~45 DEG C in temperature
Be completely dissolved mesotrione under ultrasonic wave added, add carbon modified quantum dot solution, 3- aminopropyl triethoxysilane, just
The ammonia spirit that silester and mass fraction are 20%~30%, is put into sealing container after magnetic stir bar, and be transferred to magnetic
On power blender, it is protected from light lower magnetic agitation reaction 20h~30h in room temperature, initial reaction product is obtained, initial reaction solution is existed
Revolving speed is centrifuged 5min~10min, solid product after being separated, using methanol to separation under the conditions of being 5000rpm~7000rpm
Solid product elutes 2~4 times afterwards, carries out vacuum drying 10h~15h at being then 50 DEG C~70 DEG C in temperature, obtains carbon quantum
Point-molecular imprinting composite material；The quality of mesotrione described in step 3 and the volume ratio of dehydrated alcohol are 1g:(0.075
~0.125) mL；The mass ratio of the volume of carbon modified quantum dot solution and mesotrione described in step 3 is 1mL:(3~5)
mg；The volume ratio of carbon modified quantum dot solution described in step 3 and 3- aminopropyl triethoxysilane is 1mL:(6~8) μ
L；The volume ratio of carbon modified quantum dot solution and ethyl orthosilicate described in step 3 is 1:(0.02~0.04)；In step 3
The volume ratio for the ammonia spirit that the carbon modified quantum dot solution and mass fraction is 20%~30% is 1mL:(3~5) μ L.
It is a kind of to analyze the remaining method of pesticide mesotrione using carbon quantum dot-molecular imprinting composite material, specifically press
What following steps were completed:
One, it prepares dispersion liquid: carbon quantum dot-molecular imprinting composite material being distributed in high purity water, dispersion liquid is obtained；Step
Carbon quantum dot-molecular imprinting composite material quality described in rapid one and the volume ratio of high purity water are 1mg:(0.8~1.5)
mL；
Two, detect control group fluorescence intensity: by dispersion liquid, 1:1 is uniformly mixed by volume with high purity water, obtains control group
Solution detects control group solution in the case where excitation wavelength is 350nm, launch wavelength is 453nm using sepectrophotofluorometer, obtains
Fluorescence intensity F0；
Three, quenching constant K is determinedsv: it is Q 1., by dispersion liquid and concentration1Mesotrione aqueous solution 1:1 is mixed by volume
It closes uniformly, 15nmol/L≤Q1, obtaining concentration is Q1Test group solution is in excitation wavelength using sepectrophotofluorometer
350nm, launch wavelength are that detectable concentration is Q under 453nm1Test group solution obtains fluorescence intensity F1；2., according to mesotrione water
In solution 1. mesotrione increasing concen-trations form repetition step 3 operates n-1 times, when n-th operates, in mesotrione aqueous solution
Mesotrione concentration is Qn, Qn≤ 3000nmol/L, using sepectrophotofluorometer excitation wavelength is 350nm, launch wavelength is
It is F that detection, which obtains fluorescence intensity, under 453nmn；3., according to Stern-Volmer equation be F0/ F=1+Ksv[Q], F in formula0For
The fluorescence intensity of control group solution, F are the fluorescence intensity of test group solution, F=F1~Fn, Q is test group mesotrione aqueous solution
The concentration of middle mesotrione, Q=Q1~Qn, KsvFor quenching constant Ksv, according to Q1~QnAnd F1~Fn, with F0/ F is y, Q x, Ksv
Quenching constant K is finally obtained for k, linear equation y=kx+1svValue；
Four, detect sample to be tested: by dispersion liquid, 1:1 is uniformly mixed by volume with sample to be tested, obtains to be measured group of solution,
To be measured group of solution is detected in the case where excitation wavelength is 350nm, launch wavelength is 453nm using sepectrophotofluorometer, obtains fluorescence
Intensity Fu, it is F according to Stern-Volmer equation0/Fu=1+Ksv[Qu], F in formula0For the fluorescence intensity of control group solution, Fu
For the fluorescence intensity of to be measured group of solution, KsvFor quenching constant, the concentration Q of mesotrione in sample to be tested is calculatedu。
The invention has the advantages that the mangrove bark that the raw material that the 1, present invention uses is discarded for biological material, material environmental protection, realize
Refuse reclamation, and application prospect is bigger；2, carbon quantum dot-molecular imprinting composite material synthetic method that the present invention is prepared
Simply, condition is easily controllable, and solvent for use is high purity water, reduces the use of organic solvent, and environmental pollution is small；3, present invention inspection
It surveys that the time is short, and 10min can complete to detect, there is the good rate of recovery and reproducibility, to mesotrione selectivity with higher,
Selectivity factor > 2.5, rate of recovery > 90%, RSD < 5%.
Present invention is mainly used for pesticide mesotrione residuals in analysis environmental water sample.
Detailed description of the invention
Fig. 1 is carbon quantum dot-molecular imprinting composite material Fourier transform infrared spectroscopy figure prepared by embodiment 1；
Fig. 2 is carbon quantum dot-molecular imprinting composite material x-ray photoelectron spectrogram prepared by embodiment 1；
Fig. 3 is carbon quantum dot-molecular imprinting composite material transmission electron microscope picture prepared by embodiment 1；
Fig. 4 is carbon quantum dot-molecular imprinting composite material X-ray diffraction spectrogram prepared by embodiment 1；
Fig. 5 is carbon quantum dot-molecular imprinting composite material pH value influence diagram prepared by embodiment 1；
Fig. 6 be in 2 step 3 of embodiment mesotrione aqueous solution to carbon quantum dot-molecular imprinting composite material quenching shadow
Ring figure；
Fig. 7 is Stern-Volmer Linear equations in 2 step 3 of embodiment.
Specific embodiment
Specific embodiment 1: present embodiment is a kind of preparation method of carbon quantum dot-molecular imprinting composite material, tool
Body is completed by the following steps:
One, it prepares carbon quantum dot: mangrove bark being put into polytetrafluoroethyllining lining first, high purity water is added and is uniformly mixed,
It is put into stainless steel cauldron after capping, reaction kettle is sealed, be then placed in air dry oven, be 180 DEG C~220 in temperature
3h~7h is reacted at DEG C, after being cooled to room temperature, obtains reaction product, and the micropore filtering film for being 20 μm~40 μm using aperture is to anti-
It answers product to be filtered, obtains lurid filtrate, which is carbon quantum dot solution；It is described in step 1
The quality of mangrove bark and the volume ratio of high purity water are 1g:(10~20) mL；
Two, modified carbon quantum dot: 3- aminopropyl triethoxysilane is added into carbon quantum dot solution, low whipping speed is
100rpm~300rpm and temperature are that 20h~30h is reacted at 50 DEG C~70 DEG C, and solution after being reacted exists solution after reaction
Revolving speed be 5000rpm~7000rpm under the conditions of be centrifuged 5min~10min, isolated supernatant, using ether to supernatant into
Row extraction 2~4 times, obtains carbon modified quantum dot solution；3- aminopropyl triethoxysilane and carbon quantum described in step 2
The volume ratio of point solution is 1:(22~28)；
Three, molecular engram: mesotrione is put into container, and dehydrated alcohol is then added, and is 35 DEG C~45 DEG C in temperature
Be completely dissolved mesotrione under ultrasonic wave added, add carbon modified quantum dot solution, 3- aminopropyl triethoxysilane, just
The ammonia spirit that silester and mass fraction are 20%~30%, is put into sealing container after magnetic stir bar, and be transferred to magnetic
On power blender, it is protected from light lower magnetic agitation reaction 20h~30h in room temperature, initial reaction product is obtained, initial reaction solution is existed
Revolving speed is centrifuged 5min~10min, solid product after being separated, using methanol to separation under the conditions of being 5000rpm~7000rpm
Solid product elutes 2~4 times afterwards, carries out vacuum drying 10h~15h at being then 50 DEG C~70 DEG C in temperature, obtains carbon quantum
Point-molecular imprinting composite material；The quality of mesotrione described in step 3 and the volume ratio of dehydrated alcohol are 1g:(0.075
~0.125) mL；The mass ratio of the volume of carbon modified quantum dot solution and mesotrione described in step 3 is 1mL:(3~5)
mg；The volume ratio of carbon modified quantum dot solution described in step 3 and 3- aminopropyl triethoxysilane is 1mL:(6~8) μ
L；The volume ratio of carbon modified quantum dot solution and ethyl orthosilicate described in step 3 is 1:(0.02~0.04)；In step 3
The volume ratio for the ammonia spirit that the carbon modified quantum dot solution and mass fraction is 20%~30% is 1mL:(3~5) μ L.
Specific embodiment 2: the difference of present embodiment and specific embodiment one is: being in temperature in step 1
3h is reacted at 200 DEG C.Other are same as the specific embodiment one.
Specific embodiment 3: one of present embodiment and specific embodiment one or two difference are: institute in step 1
The quality for the mangrove bark stated and the volume ratio of high purity water are 1g:15mL.Other are the same as one or two specific embodiments.
Specific embodiment 4: one of present embodiment and specific embodiment one to three difference are: in step 2
Mixing speed is 200rpm and temperature is to react for 24 hours at 60 DEG C.Other are identical as specific embodiment one to three.
Specific embodiment 5: one of present embodiment and specific embodiment one to four difference are: in step 2
Revolving speed is centrifuged 8min, isolated supernatant under the conditions of being 6000rpm.Other are identical as specific embodiment one to four.
Specific embodiment 6: one of present embodiment and specific embodiment one to five difference are: in step 3
Room temperature is protected from light lower magnetic agitation reaction 20h~30h, and the revolving speed of magnetic agitation is 200rpm~300rpm, obtains initial reaction production
Object.Other are identical as specific embodiment one to five.
Specific embodiment 7: one of present embodiment and specific embodiment one to six difference are: will in step 3
Initial reaction solution is centrifuged 8min under the conditions of revolving speed is 6000rpm, solid product after being separated.Other and specific embodiment party
Formula one to six is identical.
Specific embodiment 8: one of present embodiment and specific embodiment one to seven difference are: sharp in step 3
Solid product after separation is eluted 3 times with methanol, vacuum drying 12h is carried out at being then 60 DEG C in temperature, obtains carbon quantum dot-
Molecular imprinting composite material.Other are identical as specific embodiment one to seven.
Specific embodiment 9: present embodiment is a kind of utilization carbon quantum dot-molecular imprinting composite material analysis pesticide
The remaining method of mesotrione, is specifically realized by the following steps:
One, it prepares dispersion liquid: carbon quantum dot-molecular imprinting composite material being distributed in high purity water, dispersion liquid is obtained；Step
Carbon quantum dot-molecular imprinting composite material quality described in rapid one and the volume ratio of high purity water are 1mg:(0.8~1.5)
mL；
Two, detect control group fluorescence intensity: by dispersion liquid, 1:1 is uniformly mixed by volume with high purity water, obtains control group
Solution detects control group solution in the case where excitation wavelength is 350nm, launch wavelength is 453nm using sepectrophotofluorometer, obtains
Fluorescence intensity F0；
Three, quenching constant K is determinedsv: it is Q 1., by dispersion liquid and concentration1Mesotrione aqueous solution 1:1 is mixed by volume
It closes uniformly, 15nmol/L≤Q1, obtaining concentration is Q1Test group solution is in excitation wavelength using sepectrophotofluorometer
350nm, launch wavelength are that detectable concentration is Q under 453nm1Test group solution obtains fluorescence intensity F1；2., according to mesotrione water
In solution 1. mesotrione increasing concen-trations form repetition step 3 operates n-1 times, when n-th operates, in mesotrione aqueous solution
Mesotrione concentration is Qn, Qn≤ 3000nmol/L, using sepectrophotofluorometer excitation wavelength is 350nm, launch wavelength is
It is F that detection, which obtains fluorescence intensity, under 453nmn；3., according to Stern-Volmer equation be F0/ F=1+Ksv[Q], F in formula0For
The fluorescence intensity of control group solution, F are the fluorescence intensity of test group solution, F=F1~Fn, Q is test group mesotrione aqueous solution
The concentration of middle mesotrione, Q=Q1~Qn, KsvFor quenching constant Ksv, according to Q1~QnAnd F1~Fn, with F0/ F is y, Q x, Ksv
Quenching constant K is finally obtained for k, linear equation y=kx+1svValue；
Four, detect sample to be tested: by dispersion liquid, 1:1 is uniformly mixed by volume with sample to be tested, obtains to be measured group of solution,
To be measured group of solution is detected in the case where excitation wavelength is 350nm, launch wavelength is 453nm using sepectrophotofluorometer, obtains fluorescence
Intensity Fu, it is F according to Stern-Volmer equation0/Fu=1+Ksv[Qu], F in formula0For the fluorescence intensity of control group solution, Fu
For the fluorescence intensity of to be measured group of solution, KsvFor quenching constant, the concentration Q of mesotrione in sample to be tested is calculatedu。
Specific embodiment 10: the difference of present embodiment and specific embodiment nine is: carbon described in step 1
Quantum dot-molecular imprinting composite material quality and the volume ratio of high purity water are 1mg:1mL.Other and nine phase of specific embodiment
Together.
Using following verification experimental verifications effect of the present invention
Embodiment 1: a kind of preparation method of carbon quantum dot-molecular imprinting composite material is specifically realized by the following steps
:
One, it prepares carbon quantum dot: 2.0g mangrove bark being put into polytetrafluoroethyllining lining first, it is mixed that 30mL high purity water is added
It closes uniformly, is put into stainless steel cauldron after capping, reaction kettle is sealed, be then placed in air dry oven, be 200 in temperature
3h is reacted at DEG C, after being cooled to room temperature, obtains reaction product, and reaction product is carried out using the micropore filtering film that aperture is 22 μm
Filtering, obtains lurid filtrate, which is carbon quantum dot solution；
Two, modified carbon quantum dot: 50mL carbon quantum dot solution is added in there-necked flask, 2mL 3- aminopropyl three is then added
Ethoxysilane, low whipping speed is 200rpm and temperature is to react at 60 DEG C for 24 hours, solution after being reacted, will be molten after reaction
Liquid is centrifuged 8min under the conditions of revolving speed is 6000rpm, and isolated supernatant carries out extraction 3 times to supernatant using ether, obtains
To carbon modified quantum dot solution；
Three, molecular engram: 200mg mesotrione is put into there-necked flask, and 20mL dehydrated alcohol is then added, is in temperature
It is completely dissolved mesotrione under 40 DEG C and ultrasonic wave added, adds 50mL carbon modified quantum dot solution, 350 μ L 3- aminopropyls
The ammonia spirit that triethoxysilane, 1.5mL ethyl orthosilicate and 200 μ L mass fractions are 25%, after being put into magnetic stir bar
There-necked flask is sealed, and is transferred on magnetic stirring apparatus, is protected from light lower magnetic agitation reaction for 24 hours in room temperature, the revolving speed of magnetic agitation is
250rpm obtains initial reaction product, and initial reaction solution is centrifuged 8min under the conditions of revolving speed is 6000rpm, is separated
Solid product afterwards elutes solid product after separation 3 times using methanol, carries out vacuum drying 12h at being then 60 DEG C in temperature,
Obtain carbon quantum dot-molecular imprinting composite material；
Carbon quantum dot-the molecular imprinting composite material prepared using Fourier's IR Characterization embodiment 1, as shown in Figure 1, figure
1 is carbon quantum dot-molecular imprinting composite material Fourier transform infrared spectroscopy figure prepared by embodiment 1；Exist as shown in Figure 1
1124cm-1And 1050cm-1The strong broad peak of left and right is the asymmetric stretching vibration peak of Si-O-Si and Si-O-C, in 448cm-1With
784cm-1Place shows the vibration peak of Si-O key；In 1652cm-1The peak of left and right is the characteristic absorption peak of C=O；In 2936cm-1It is left
Right peak is the vibration absorption peak of C-H.3440cm-1The peak of left and right is N-H vibration absorption peak.
Fig. 2 is carbon quantum dot-molecular imprinting composite material x-ray photoelectron spectrogram prepared by embodiment 1；It is penetrated by X
Photoelectron spectrogram measures the surface-element analysis of resulting materials.Carbon quantum dot-molecular imprinting composite material prepared by embodiment 1
Gamut x-ray photoelectron spectrum analysis clearly demonstrate 289.9ev, 406.1ev, 538.8ev, 108.4ev and
Five peaks of 160.4ev, respectively due to C1s, N1s, O1s, Si2p and Si2s.Illustrate the element composition and nitre sulphur of material
Humulone is all eluted.
Fig. 3 is carbon quantum dot-molecular imprinting composite material transmission electron microscope picture prepared by embodiment 1；Transmission electron microscope can be with
For observing pattern, You Tuke 3 knows, carbon quantum dot-molecular imprinting composite material is chondritic, and diameter is about 30~50nm,
Regular shape and good dispersion.
Fig. 4 is carbon quantum dot-molecular imprinting composite material X-ray diffraction spectrogram prepared by embodiment 1；X-ray diffraction
Spectrogram can reflect crystals Atomic Arrangement rule, as can be seen from Figure 42 θ within the scope of 15 ° -40 ° there are one very
Wide diffraction maximum, corresponding carbon quantum dot-molecular imprinting composite material diffraction crystal face.Carbon quantum dot-molecular imprinting composite material
002 crystal face is very wide, this illustrates that a kind of state of longrange disorder is presented in product.Carbon in transmission electron microscope picture in this result and Fig. 3
Quantum dot-molecular imprinting composite material shape characteristic is consistent.
Fig. 5 is carbon quantum dot-molecular imprinting composite material pH value influence diagram prepared by embodiment 1；As shown in Figure 5, pH
Carbon quantum dot-molecular imprinting composite material fluorescence intensity slightly fluctuates when value is 3~12, but whole relatively stable, shows carbon amounts
Sub- point-molecular imprinting composite material has very strong stability.
Embodiment 2: it is a kind of to analyze the remaining method of pesticide mesotrione using carbon quantum dot-molecular imprinting composite material,
It is specifically realized by the following steps:
One, it prepares dispersion liquid: carbon quantum dot-molecular imprinting composite material being distributed in high purity water, dispersion liquid is obtained；Step
Carbon quantum dot-molecular imprinting composite material quality described in rapid one and the volume ratio of high purity water are 1mg:1mL；
Two, it detects control group fluorescence intensity: 1.5mL dispersion liquid being uniformly mixed with 1.5mL high purity water, it is molten to obtain control group
Liquid detects control group solution in the case where excitation wavelength is 350nm, launch wavelength is 453nm using sepectrophotofluorometer, obtains glimmering
Luminous intensity F0, F0=3197；
Three, quenching constant K is determinedsv: it is Q 1., by 1.5mL dispersion liquid and 1.5mL concentration1Mesotrione aqueous solution mixing
Uniformly, Q1=15nmol/L, obtaining concentration is Q1Test group solution, using sepectrophotofluorometer excitation wavelength be 350nm,
Launch wavelength is that detectable concentration is Q under 453nm1Test group solution obtains fluorescence intensity F1；2., successively using concentration be Q2~Q11
Mesotrione aqueous solution replacement concentration be Q1Mesotrione aqueous solution repeat step 3 1. operate 10 times；Q2=
313.5nmol/L, fluorescence intensity F2；Q3=612nmol/L, fluorescence intensity F3；Q4=910.5nmol/L, fluorescence intensity are
F4；Q5=1209nmol/L, fluorescence intensity F5；Q6=1507.5nmol/L, fluorescence intensity F6；Q7=1806nmol/L, it is glimmering
Luminous intensity is F7；Q8=2104.5nmol/L, fluorescence intensity F8；Q9=2403nmol/L, fluorescence intensity F9；Q10=
2701.5nmol/L fluorescence intensity F10；Q11=3000nmol/L, fluorescence intensity F11；3., according to the side Stern-Volmer
Journey is F0/ F=1+Ksv[Q], F in formula0For the fluorescence intensity of control group solution, F is the fluorescence intensity of test group solution, F=F1
~F11, Q is the concentration of mesotrione in test group mesotrione aqueous solution, Q=Q1~Q11, KsvFor quenching constant Ksv, according to Q1
~Q11And F1~F11, with F0/ F is y, Q x, KsvY=is obtained by the Fitting Calculation for k, linear equation y=kx+1
7.363×10-4x+1(R2=0.99) quenching constant K, is finally obtainedsv=7.363 × 10-4；
Four, it detects sample to be tested: 1.5mL dispersion liquid being uniformly mixed with 1.5mL sample to be tested, obtains to be measured group of solution,
To be measured group of solution is detected in the case where excitation wavelength is 350nm, launch wavelength is 453nm using sepectrophotofluorometer, obtains fluorescence
Intensity Fu, it is F according to Stern-Volmer equation0/Fu=1+Ksv[Qu], F in formula0For the fluorescence intensity of control group solution, Fu
For the fluorescence intensity of to be measured group of solution, KsvFor quenching constant, the concentration Q of mesotrione in sample to be tested is calculatedu=22nmol/
L；The sample to be tested is the mesotrione aqueous solution that concentration is 22nmol/L.
Fig. 6 be in 2 step 3 of embodiment mesotrione aqueous solution to carbon quantum dot-molecular imprinting composite material quenching shadow
Ring figure；Mesotrione aqueous solution of the concentration between 15nmol/L~3000nmol/L is used to utilize in the present embodiment step 3
Stern-Volmer equation analyzes (as shown in Figure 7) experimental data, and Fig. 7 is Stern- in 2 step 3 of embodiment
Volmer Linear equations；There is good linear relationship, linear equation y between concentration 15nmol/L~3000nmol/L
=7.363 × 10-4x+1(R2=0.99).
Claims (10)
1. a kind of preparation method of carbon quantum dot-molecular imprinting composite material, which is characterized in that the preparation method presses following step
It is rapid to complete:
One, it prepares carbon quantum dot: mangrove bark being put into polytetrafluoroethyllining lining first, high purity water is added and is uniformly mixed, covers
After be put into stainless steel cauldron, reaction kettle is sealed, is then placed in air dry oven, temperature be 180 DEG C~220 DEG C at
3h~7h is reacted, after being cooled to room temperature, obtains reaction product, reaction is produced using the micropore filtering film that aperture is 20 μm~40 μm
Object is filtered, and obtains lurid filtrate, which is carbon quantum dot solution；Mango described in step 1
The quality of skin and the volume ratio of high purity water are 1g:(10~20) mL；
Two, modified carbon quantum dot: 3- aminopropyl triethoxysilane is added into carbon quantum dot solution, low whipping speed is
100rpm~300rpm and temperature are that 20h~30h is reacted at 50 DEG C~70 DEG C, and solution after being reacted exists solution after reaction
Revolving speed be 5000rpm~7000rpm under the conditions of be centrifuged 5min~10min, isolated supernatant, using ether to supernatant into
Row extraction 2~4 times, obtains carbon modified quantum dot solution；3- aminopropyl triethoxysilane and carbon quantum described in step 2
The volume ratio of point solution is 1:(22~28)；
Three, molecular engram: mesotrione is put into container, and dehydrated alcohol is then added, for 35 DEG C~45 DEG C and super in temperature
It is completely dissolved mesotrione under sound auxiliary, adds carbon modified quantum dot solution, 3- aminopropyl triethoxysilane, positive silicic acid
The ammonia spirit that ethyl ester and mass fraction are 20%~30%, is put into sealing container after magnetic stir bar, and be transferred to magnetic force and stir
It mixes on device, is protected from light lower magnetic agitation reaction 20h~30h in room temperature, initial reaction product is obtained, by initial reaction solution in revolving speed
To be centrifuged 5min~10min, solid product after being separated, using methanol to solid after separation under the conditions of 5000rpm~7000rpm
Body product elution 2~4 times, vacuum drying 10h~15h is carried out at being then 50 DEG C~70 DEG C in temperature, obtains carbon quantum dot-point
Sub- trace composite material；The quality of mesotrione described in step 3 and the volume ratio of dehydrated alcohol be 1g:(0.075~
0.125)mL；The mass ratio of the volume of carbon modified quantum dot solution and mesotrione described in step 3 is 1mL:(3~5)
mg；The volume ratio of carbon modified quantum dot solution described in step 3 and 3- aminopropyl triethoxysilane is 1mL:(6~8) μ
L；The volume ratio of carbon modified quantum dot solution and ethyl orthosilicate described in step 3 is 1:(0.02~0.04)；In step 3
The volume ratio for the ammonia spirit that the carbon modified quantum dot solution and mass fraction is 20%~30% is 1mL:(3~5) μ L.
2. a kind of preparation method of carbon quantum dot-molecular imprinting composite material according to claim 1, it is characterised in that step
3h is reacted at being 200 DEG C in temperature in rapid one.
3. a kind of preparation method of carbon quantum dot-molecular imprinting composite material according to claim 1, it is characterised in that step
The quality of mangrove bark described in rapid one and the volume ratio of high purity water are 1g:15mL.
4. a kind of preparation method of carbon quantum dot-molecular imprinting composite material according to claim 1, it is characterised in that step
Low whipping speed is 200rpm in rapid two and temperature is to react for 24 hours at 60 DEG C.
5. a kind of preparation method of carbon quantum dot-molecular imprinting composite material according to claim 1, it is characterised in that step
8min, isolated supernatant are centrifuged under the conditions of revolving speed is 6000rpm in rapid two.
6. a kind of preparation method of carbon quantum dot-molecular imprinting composite material according to claim 1, it is characterised in that step
It is protected from light lower magnetic agitation reaction 20h~30h in room temperature in rapid three, the revolving speed of magnetic agitation is 200rpm~300rpm, is obtained just
Walk reaction product.
7. a kind of preparation method of carbon quantum dot-molecular imprinting composite material according to claim 1, it is characterised in that step
Initial reaction solution is centrifuged 8min under the conditions of revolving speed is 6000rpm in rapid three, solid product after being separated.
8. a kind of preparation method of carbon quantum dot-molecular imprinting composite material according to claim 1, it is characterised in that step
Solid product after separation is eluted 3 times using methanol in rapid three, vacuum drying 12h is carried out at being then 60 DEG C in temperature, obtains
Carbon quantum dot-molecular imprinting composite material.
9. a kind of analyze the remaining method of pesticide mesotrione using carbon quantum dot-molecular imprinting composite material, which is characterized in that
Carbon quantum dot-the molecular imprinting composite material being prepared using claim 1, and complete according to the following steps:
One, it prepares dispersion liquid: carbon quantum dot-molecular imprinting composite material being distributed in high purity water, dispersion liquid is obtained；Step 1
Described in carbon quantum dot-molecular imprinting composite material quality and high purity water volume ratio be 1mg:(0.8~1.5) mL；
Two, detect control group fluorescence intensity: by dispersion liquid, 1:1 is uniformly mixed by volume with high purity water, obtains control group solution,
Control group solution is detected in the case where excitation wavelength is 350nm, launch wavelength is 453nm using sepectrophotofluorometer, obtains fluorescence
Intensity F0；
Three, quenching constant K is determinedsv: it is Q 1., by dispersion liquid and concentration1The 1:1 mixing by volume of mesotrione aqueous solution it is equal
It is even, 15nmol/L≤Q1, obtaining concentration is Q1Test group solution is 350nm, sends out using sepectrophotofluorometer in excitation wavelength
Detectable concentration is Q under a length of 453nm of ejected wave1Test group solution obtains fluorescence intensity F1；2., according to nitre in mesotrione aqueous solution
Sulphur humulone increasing concen-trations form repeats step 3 and 1. operates n-1 times, when n-th operates, mesotrione in mesotrione aqueous solution
Concentration is Qn, Qn≤ 3000nmol/L, using sepectrophotofluorometer in the case where excitation wavelength is 350nm, launch wavelength is 453nm
It is F that detection, which obtains fluorescence intensity,n；3., according to Stern-Volmer equation be F0/ F=1+Ksv[Q], F in formula0It is molten for control group
The fluorescence intensity of liquid, F are the fluorescence intensity of test group solution, F=F1~Fn, Q is nitre sulphur grass in test group mesotrione aqueous solution
The concentration of ketone, Q=Q1~Qn, KsvFor quenching constant Ksv, according to Q1~QnAnd F1~Fn, with F0/ F is y, Q x, KsvFor k, fitting
Linear equation y=kx+1 finally obtains quenching constant KsvValue；
Four, detect sample to be tested: by dispersion liquid, 1:1 is uniformly mixed by volume with sample to be tested, obtains to be measured group of solution, is utilized
Sepectrophotofluorometer detects to be measured group of solution in the case where excitation wavelength is 350nm, launch wavelength is 453nm, obtains fluorescence intensity
Fu, it is F according to Stern-Volmer equation0/Fu=1+Ksv[Qu], F in formula0For the fluorescence intensity of control group solution, FuFor to
The fluorescence intensity of survey group solution, KsvFor quenching constant, the concentration Q of mesotrione in sample to be tested is calculatedu。
10. according to claim 9 a kind of residual using carbon quantum dot-molecular imprinting composite material analysis pesticide mesotrione
The method stayed, it is characterised in that the quality of carbon quantum dot-molecular imprinting composite material described in step 1 and the body of high purity water
Product is than being 1mg:1mL.
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